• Title/Summary/Keyword: Liquid Liquid Extraction

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Evaluation on Extraction Conditions and HPLC Analysis Method for Ginsenosides in Panax ginseng (인삼의 추출조건 및 진세노사이드의 HPLC 분석법 평가)

  • Lee, Kyeong Hee;Lee, Dae Young;Lee, Seung Eun;Nam, Ki Yeul;Hwang, Gwang Bo;Kim, Hyung Don;Lee, Jae Won;Choi, Je Hun;Ahn, Young Sup;Kim, Seung Yu;Kim, Geum Soog
    • Korean Journal of Medicinal Crop Science
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    • v.24 no.1
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    • pp.47-54
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    • 2016
  • Background : A new extraction method-heated ultrasonic extraction was qualitatively and quantitatively analyzed for the extraction of major ginsenosides from ginseng extract; this new high-performance liquid chromatography (HPLC) method was compared with the official extraction method of Korean industrial standards and standard for health functional food. Methods and Results : Ginsenoside compounds were analyzed for 35 minutes by the new HPLC analysis method using a Halo$^{(R)}$ RP-Amide column. The new HPLC analysis method was validated by the measurement of intra-day and inter-day precision, accuracy, limit of detection (LOD), and limit of quantification (LOQ) of each ginsenoside. The correlation coefficients (r2) for the calibration curves of the ginsenoside compounds were over 0.9997 in terms of linearity. The heated ultrasonic extraction method using ultrasonication for 30 minutes at $50^{\circ}C$ yielded higher amount of ginsenosides than the extraction method of the Korean industrial standards owing to the enhancement of extraction efficiency. Conclusions : Compared to the other extraction methods, the heated ultrasonic extraction method yielded a higher amount of ginsenoside Rb1 than Rg1 index compounds for the quality evaluation of ginseng roots.

Compositional differences of Bojungikgi-tang decoctions using pressurized or non-pressurized extraction methods with variable extraction times

  • Kim, Jung-Hoon;Seo, Chang-Seob;Kim, Seong-Sil;Shin, Hyeun-Kyoo
    • The Korea Journal of Herbology
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    • v.28 no.4
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    • pp.1-6
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    • 2013
  • Objectives : In other to determine the optimal extraction conditions, the various Bojungikgi-tang (BJIGT) decoctions prepared by different pressure levels and different extraction times were compared and evaluated in terms of the extract yield and the total soluble solid content. Methods : Decoctions were prepared by the pressure levels of 0 (non-pressurized) and 1 $kgf/cm^2$ (pressurized) for 60, 120 and 180 min. The extract yield and the total soluble solids content of decoctions were measured, and the amounts of the reference compounds in decoctions were investigated by the analysis using high performance liquid chromatography. Results : The extract yield and the total soluble solid content were higher in decoctions extracted by the pressurized method than those from decoction with non-pressurized method. The patterns of yield and contents showed a proportional increase to the extraction time. In analysis of the linear regression for four reference compounds such as liquiritin, nodakenin, hesperidin, and glycyrrhizin, the good linearity with the correlation coefficient more than 0.9999 was observed. The highest contents for four reference compounds were observed at 180 min of both the pressurized method and the non-pressurized method. Conclusions : This study suggests that the pressure in extraction method and the extraction time affect the compositional constituents in BJIGT decoctions. The extraction time of 180 min could be chosen in both pressurized and non-pressurized method as optimal extraction condition.

Separation Behavior of Paclitaxel and Its Semi-synthetic Precursor 10-Deacetylpaclitaxel from Plant Cell Cultures (식물세포배양으로부터 파클리탁셀 및 이의 반합성 전구체 10-디아세틸파클리탁셀의 분리 양상)

  • Lee, Chung-Gi;Kim, Jin-Hyun
    • Korean Chemical Engineering Research
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    • v.54 no.1
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    • pp.89-93
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    • 2016
  • In this study, we investigated the separation behavior of the anticancer agent paclitaxel and its semi-synthetic precursor 10-deacetylpaclitaxel (10-DAP) from plant cell cultures. As a result of sequential separation/purification performed by biomass extraction with solvent, liquid-liquid extraction, adsorbent treatment, hexane precipitation, and fractional precipitation, the adsorbent treatment was found to be the most effective in separating and recovering 10-DAP from paclitaxel. The optimal adsorbent type, crude extract/adsorbent ratio, and adsorbent treatment temperature were sylopute, 1:1.5 (w/w), and $20^{\circ}C$, respectively. The separation/recovery of 10-DAP from paclitaxel was 74.1% in adsorbent treatment process under optimal conditions.

Sample Pretreatment and HRGC/HRMS Analysis for Determination of Dioxins in Environmental Samples (환경시료 중 다이옥신류의 정량을 위한 시료전처리방법의 개선 및 고분해능 GC/MS 분석에 관한 연구 Ⅰ)

  • Kim, Jin Yeong;Jang, Yun Seok;Lee, Dae Un
    • Journal of the Korean Chemical Society
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    • v.38 no.11
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    • pp.819-826
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    • 1994
  • This study described a simple, rapid and cost effective analytical technique for the ultra-trace analysis of dioxins in environmental samples. Liquid-Liquid extraction methods were used for the initial extraction and enrichment of the analyte. Subsequent clean-up procedures were achieved by using strong cation exchanger, silica and Florisil cartridges. Extracts were analysed by HRGC/HRMS-SIM. The efficiency of these analytical methods was tested by recovery and selectivity for elimination of interferences such as phenols, pesticides and PCBs in each step. The mean recovery of 1,2,3,4-TCDD spiked at 10 ppt in sea water was about 92(${\pm}$1.6)%. This analytical method was applied to Kwangyang sea water and 4.5pg/L of 2,3,7,8-TCDD was determined.

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Extraction of Phthalate Esters in Environmental Water Samples Using Layered-Carbon Magnetic Hybrid Material as Adsorbent Followed by Their Determination with HPLC

  • Wang, Weina;Wu, Qiuhua;Zang, Xiaohuan;Wang, Chun;Wang, Zhi
    • Bulletin of the Korean Chemical Society
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    • v.33 no.10
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    • pp.3311-3316
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    • 2012
  • In this paper, a layered-carbon-$Fe_3O_4$ (LC-$Fe_3O_4$) hybrid material was synthesized through a facile one-pot solvothermal method and used as the adsorbent for the preconcentration of some phthalate esters (dimethyl phthalate, diethyl phthalate, diallyl phthalate, diisobutyl phthalate and benzyl butyl phthalate) in water samples. The effects of the adsorbent dosage, extraction time, the solution pH and salinity on the adsorption of the phthalate esters (PAEs) were investigated. The magnetic nanocomposite adsorbent could remove and enrich the PAEs from water samples efficiently. After the adsorption, the analytes were desorbed and then determined by high performance liquid chromatography-ultraviolet detection. Under the optimum conditions, the enrichment factors of the method for the analytes were in the range from 161 to 180. A linear response with peak area as the quantification signal was observed in the concentration range from 0.5 to $100ng\;mL^{-1}$. The limits of detection (S/N = 3) of the method were between 0.08 and $0.1ng\;mL^{-1}$. The method was suitable for the determination of trace phthalate esters in environmental water samples.

A Study on the Mass Transfer of Extraction Process by Use of Hollow Fiber Membrane Module (실관막 모듈을 이용한 추출공정의 물질전달에 관한 연구)

  • Kim, Young-Il;Jin, Do-Won;Kim, Jong-Hyun;Choi, Dai-Ung;Park, Dong-Won
    • Applied Chemistry for Engineering
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    • v.7 no.5
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    • pp.977-984
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    • 1996
  • Liquid-liquid extractions by use of hollow fiber membrane module are fast because of the large surface area per volume. In these membranes, the extractant and feed can be contacted at high speed and two flows are completely independent, so there are no problems with loading and channeling. In this paper, it was investigated the selectivities of extractants for extraction of heavy metals from aqueous solution into organic extractants by using the hollow fiber membrane. To identify the effect of distribution ratio on mass transfer in the membrane, we also compared the distribution ratio with mass transfer coefficient. From these experiments for the system with high distribution ratio, effect of the distribution ratio on mass transfer was weak compare with the low distribution ratio system in the hollow fiber membrane.

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Optimization Condition of Trace Analysis of Fuel Oxygenated Compounds Using The Design of Experiment (DOE) in Solid-Phase Microextraction with GC/FID (고체상미량분석법(SPME-GC/FID)에서 실험계획법을 이용한 연료첨가제 미량분석의 최적조건)

  • An, Sang-Woo;Lee, Si-Jin;Chang, Soon-Woong
    • Journal of Soil and Groundwater Environment
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    • v.15 no.1
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    • pp.9-18
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    • 2010
  • In this study, Solid-phase micro-extraction (SPME) with Gas Chromatograph using Flame Ionization Detector (GC/FID) was studied as a possible alternative to liquid-liquid extraction for the analysis of Methyl tert-butyl ether (MTBE) and Tertiary-butyl ether (TBA) in water and an optimization condition of trace analysis of MTBE and TBA using the design of experiment (DOE) was described. The aim of our research was to apply experimental design methodology in the optimization condition of trace analysis of fuel oxygenated compounds in soil-phase microextraction with GC/FID. The reactions of SPME were mathematically described as a function of parameters of Temp ($X_1$), Volume ($X_2$), Time ($X_3$) and Salt ($X_4$) being modeled by the use of the partial factorial designs, which was used for fitting 2nd order response surface models and was alternative to central composite designs. The model predicted agreed with the experimentally observed result ($Y_1$(MTBE, $R^2$ = 0.96, $Y_2$ (TBA, $R^2$ = 0.98)). The estimated ridge of the expected maximum responses and optimal conditions for MTBE and TBA were 278.13 and (Temp ($X_1$) = $48.40^{\circ}C$, Volume ($X_2$) = 73.04 mL, Time ($X_3$) = 11.51 min and Salt ($X_4$) = 12,50 mg/L), and 127.89 and (Temp ($X_1$) = $52.12^{\circ}C$, Volume ($X_2$) = 88.88mL, Time ($X_3$) = 65.40 min and Salt ($X_4$) = 12,50 mg/L), respectively.

The rapid determination of PAHs in foods using ultra high performance liquid chromatography (UHPLC를 이용한 식품 중의 PAHs 신속분석법)

  • Ha, Jae-Ho;Shin, Dong-Bin;Hwang, Jin-Bong;Seo, Hye-Young;Ito, Masahito;Nakagawa, Hiroaki
    • Analytical Science and Technology
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    • v.24 no.4
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    • pp.266-274
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    • 2011
  • Using a Hitachi LaChrom Ultra 2000U, a reverse phase ultra high performance liquid chromatography (u-HPLC) method was developed for the rapid quantification of 14 PAHs in foods. The proposed method for PAH analysis is based on solid phase extraction (SPE) cartridges; the determination was carried out by u-HPLC with fluorimetric detection. The method was very sensitive; PAH concentration levels were in a low ${\mu}g$/kg range and could be detected and quantified. Six samples of food were analyzed. Among PAHs, PHE was found in most of samples, the concentration ranging from 2.5 to 19.9 ${\mu}g$/kg. The contents of benzo[c]fluorine (BCL), pyrene (PYR), benzo[a]anthracene (BaA), chrysene (CHR), benzo[b]fluoranthene (BbF), benzo[k]fluoranthene (BkF) were low at the '${\mu}g$/kg' level or were less than LOD.

Determination of Dibutyltin in Sediments Using Isotope Dilution Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry

  • Yim, Yong-Hyeon;Park, Ji-Youn;Han, Myung-Sub;Park, Mi-Kyung;Kim, Byung-Joo;Lim, Young-Ran;Hwang, Eui-Jin;So, Hun-Young
    • Bulletin of the Korean Chemical Society
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    • v.26 no.3
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    • pp.440-446
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    • 2005
  • A method is described for the determination of dibutyltin (DBT) in sediment by isotope dilution using liquid chromatography inductively-coupled plasma/mass spectrometry (LC-ICP/MS). To achieve the highest accuracy and precision, special attentions are paid in optimization and evaluation of overall processes of the analysis including extraction of analytes, characterization of the standards used for calibration and LC-ICP/MS conditions. An approach for characterization of natural abundance DBT standard has been developed by combining inductively-coupled plasma/optical emission spectrometry (ICP/OES) and LC-ICP/MS for the total Sn assay and the analysis of Sn species present as impurities, respectively. An excellent LC condition for separation of organotin species was found, which is suitable for simultaneous DBT and tributyltin (TBT) analysis as well as impurity analysis of DBT standards. Microwave extraction condition was also optimized for high efficiency while preventing species transformation. The present method determines the amount contents of DBT in sediments with expanded uncertainty of less than 5% and its result shows high degree of equivalence with reference values of an international inter-comparison and a certified reference material (CRM) within stated uncertainties.

Determination of Phthalate Esters and Adipate in Water and Sediment Samples (수질 및 저질중의 프탈산 에스테르와 아디피산 분석)

  • Myung, Seung-Woon;Chang, Yoon-Jung;Min, Hye-Ki;Kim, Myung-Soo
    • Analytical Science and Technology
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    • v.13 no.5
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    • pp.616-623
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    • 2000
  • The most common phthalate acid esters (8 compounds) and adipate were determined from water and sediment simultaneously. After liquid-liquid extraction with n-hexane for water and sonication extraction with dichloromethane for sediment, these were determined by the GC/MS with SIM mode. There were good linearities (above $R^2=0.993$) on the range of the 0.1-20 ng/ml (water) and 10-500 ng/g (sediment), and the detection limits of method were below 0.1 ng/ml and 10 ng/g for water samples and sediment samples, respectively. The method shows a good precision and accuracy for measurement of phthalates and adipate.

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